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A combination of the evaporation-grinding MALDI-TOF MS sample preparation method with surface-modification techniques is presented for the characterization of intractable poly(p-phenylene sulfide)s (PPS). Studies focus on the relationships between the following experiments: (1) effects of MALDI laser fluence and area of irradiation on model PPS phenyl-capped trimers and cyclics; (2) modification of PPS synthesis conditions; (3) thermal curing of PPS under various atmospheric (N 2 and air) and thermal (100-300 °C) conditions; and (4) heated N-methyl-2-pyrrolidone fractionation of high MW PPS (25, 50, 75, and 100 °C). These studies yielded a wealth of information on the mass, structure, and end groups of species generated in the synthesis, postsynthesis modification, and thermal curing of PPS. Furthermore, surfacemodified MALDI sample preparation techniques were shown to selectively isolate cyclic species from high-molecular-weight PPS.

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